Revealing full chemical forms of lead in wine with combined XRF-NMR technologies

Abstract

Since 1953, The World Organization of Vine and Wine (OIV) Member States have reduced the lead maximum limits (ML) in wines, down to 0.05 mg/L (2018). Evidently, this ML value is too restrictive for wine industry as it excludes from international market a significant portion of wine production. Currently, the Codex Committee on Contaminants in Foods and OIV had recognized the value of gathering robust and novel data to better assess the best lowest ML for wine industry. Currently, there is not a direct statement within international reference documents, of which chemical form of lead must be controlled and/ or reduced. This work presents for the first time a method combining Energy Dispersive X-Ray analysis (EDAX) and Nuclear Magnetic Resonance (NMR) spectroscopies in order to determine presence and concentrations of major and trace elements of lead and other element moieties in wine that can allow to better redefine lead's ML. By identification of K, L, M, radiation shells with additional αβi labelling of lead's major and minor components with semi-quantitative XRF, combined with chemical-shift analysis of inorganic Pb4+, Pb2+ and/or organo-lead within wine samples, we propose a full discrimination framework to disentangle and quantify different chemical forms of lead.